EP0849625A1 - Thermographic imaging composition and element comprising said composition - Google Patents
Thermographic imaging composition and element comprising said composition Download PDFInfo
- Publication number
- EP0849625A1 EP0849625A1 EP97203852A EP97203852A EP0849625A1 EP 0849625 A1 EP0849625 A1 EP 0849625A1 EP 97203852 A EP97203852 A EP 97203852A EP 97203852 A EP97203852 A EP 97203852A EP 0849625 A1 EP0849625 A1 EP 0849625A1
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- EP
- European Patent Office
- Prior art keywords
- reducing agent
- imaging
- layer
- composition
- joules
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000003384 imaging method Methods 0.000 claims abstract description 25
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- 229940075579 propyl gallate Drugs 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
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- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 1
- 229940081974 saccharin Drugs 0.000 description 1
- 235000019204 saccharin Nutrition 0.000 description 1
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
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- 150000003378 silver Chemical class 0.000 description 1
- YRSQDSCQMOUOKO-KVVVOXFISA-M silver;(z)-octadec-9-enoate Chemical compound [Ag+].CCCCCCCC\C=C/CCCCCCCC([O-])=O YRSQDSCQMOUOKO-KVVVOXFISA-M 0.000 description 1
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- 229920001059 synthetic polymer Polymers 0.000 description 1
- 239000004250 tert-Butylhydroquinone Substances 0.000 description 1
- 235000019281 tert-butylhydroquinone Nutrition 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229920003176 water-insoluble polymer Polymers 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/494—Silver salt compositions other than silver halide emulsions; Photothermographic systems ; Thermographic systems using noble metal compounds
- G03C1/498—Photothermographic systems, e.g. dry silver
- G03C1/49827—Reducing agents
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/494—Silver salt compositions other than silver halide emulsions; Photothermographic systems ; Thermographic systems using noble metal compounds
- G03C1/498—Photothermographic systems, e.g. dry silver
- G03C1/4989—Photothermographic systems, e.g. dry silver characterised by a thermal imaging step, with or without exposure to light, e.g. with a thermal head, using a laser
Definitions
- the present invention relates to thermographic compositions and elements for use in direct thermal imaging.
- Thermal imaging is a process in which images are recorded by the use of imagewise modulated thermal energy.
- thermal recording processes one in which the image is generated by thermally activated transfer of a light absorbing material, the other generates the light absorbing species by thermally activated chemical or physical modification of components of the imaging medium.
- thermal imaging methods is found in "Imaging Systems" by K.I. Jacobson R.E.Jacobson - Focal Press 1976.
- Thermal energy can be delivered in a number of ways, for example by direct thermal contact or by absorption of electromagnetic radiation.
- radiant energy include infrared lasers.
- Modulation of thermal energy can be by intensity or duration or both.
- a thermal print head comprising microscopic resistor elements is fed pulses of electrical energy which are converted into heat by the Joule effect.
- the pulses are of fixed voltage and duration and the thermal energy delivered is then controlled by the number of such pulses sent.
- Radiant energy can be modulated directly by means of the energy source e.g. the voltage applied to a solid state laser.
- Direct imaging by chemical change in the imaging medium usually involves an irreversible chemical reaction which takes place very rapidly at elevated temperatures - say above 100°C - but at room temperature the rate is orders of magnitude slower such that effectively the material is stable.
- a particularly useful direct thermal imaging element uses an organic silver salt in combination with a reducing agent.
- a reducing agent such systems are often referred to as 'dry silver'.
- the chemical change induced by the application of thermal energy is the reduction of the transparent silver salt to a metallic silver image.
- Prior art thermal imaging elements tend to have a relatively low dynamic range or relatively a narrow latitude which limits the number of tones or levels of gray that can be recorded.
- thermographic imaging element comprising:
- This invention provides a heat-sensitive recording material suitable for direct thermal imaging having a high dynamic range (Dmax ⁇ 2.5, Dmin ⁇ 0.1, as described hereinafter) and a wide latitude (E1 - E2, as described hereinafter) such that a large number of tones or levels of gray can be recorded.
- Figure 1 shows the characteristic sensitometric curves obtained by plotting image density (D) versus the imaging thermal energy expressed as the number of thermal pulses applied. Labels identify the examples as high activity (H1 through H5) and low activity (L1 through L3) as shown in Tables 1 & 2.
- Figure 2 shows a sensitometric curve showing E1, E2, D min and D max .
- FIGS 3 - 7 show sensitometric curves obtained, as set forth in more detail below, from thermographic imaging materials in accordance with this invention (D1 through D15) and comparison materials (C1 through C5).
- thermographic element and composition according to the invention comprise an oxidation-reduction image-forming composition which contains a silver salt, a high activity reducing agent, as defined herein) and a low activity reducing agent ( as defined herein).
- the oxidizing agent is preferably a silver salt. of an organic acid.
- Suitable silver salts include, for example, silver behenate, silver stearate, silver oleate, silver laureate, silver hydroxy stearate, silver caprate, silver myristate, silver palmitate silver benzoate, silver benzotriazole, silver terephthalate, silver phthalate saccharin silver, phthalazionone silver, benzotriazole silver, silver salt of 3-(2-carboxyethyl-4-4-hydroxymethyl-4-thiazoline-2-thione, silver salt of 3- mercapto-4-phenyl-1,2,4-triazole and the like. In most instances silver behenate is most useful.
- reducing agents can be employed in the imaging composition of the invention.
- Typical reducing agents which can be used include, for example:
- a test formulation containing the following activity formulation #1 is prepared.
- ACTIVITY FORMULATION #1 SILVER BEHENATE 0.88 millimole/sq.ft. (9.7 millimole/sq.m.) POLY(VINYL BUTYRAL) 400 mg/sq.ft. (4400mg/ sq.m.) SUCCINIMIDE 0.25 millimole/sq.ft. (2.75 millimole/ sq.m.) TEST REDUCING AGENT 0.75 millimole / sq. ft. (8.25 millimole/ sq.m.)
- the formulation is coated on a support and is thermally imaged using a thin film thermal head in contact with a combination of the imaging medium and a protective film of 6 micron thickness polyester sheet. Contact of the head to the element is maintained by an applied pressure of 313 g/cm heater line.
- the line write time is 15 millisec. broken up into 255 increments corresponding to the pulse width referred to above. Energy per pulse is 0.041 Joule/sq.cm.
- Individual picture elements are of a size corresponding to 300 dots per inch.
- the thermal sensitive coatings are treated with a linearly increasing pattern of pulses from 5 to 255 in 10 pulse increments. Densities of the resulting image steps are measured with an X-Rite 361 densitometer in the 'ortho' mode. In the activity determination for low activity reducing agents, an additional test in which the average printing energy per pulse is increased to 0.085 Joules per sq. cm is required to generate sufficient density in the case of the low activity reducing agents. Measured activity values for high activity reducing agents, are the same in both tests. Plots of density versus pulse count can then be generated and the activity, E1, the 'toe' of the curve, i.e., the onset of image density, can be read from the plot. The practical measure of E1 is the thermal energy which generates a density 0.1 greater than Dmin. Energy can be converted from pulse count to Joules/sq.cm. using the factors given above.
- Preferred high activity reducing agents have an activation energy of less than about 6 Joules/sq. cm.
- the high activity reducing agent has an activation energy between about 1 and 10 Joules/sq. cm. and preferably between about 3 and about 6 Joules/sq. cm.
- Low activity reducing agents have an activity, as defined herein, of equal to or greater than 10 Joules/sq. cm.
- the low activity reducing agents preferably have an activity between about 10 and about 20 Joules/sq. cm., more preferably between about 10 and about 15 Joules/sq.cm.
- Figure 1 shows the characteristic sensitometric curves obtained by plotting image density (D) versus the imaging thermal energy expressed as the number of thermal pulses applied. Labels identify the examples as high activity (H1 through H5) and low activity (L1 through L3) as shown in Tables 1 & 2.
- the D max , D min , E1, and E2 values can also be obtained.
- the plots of density versus pulse count also provides contrast and tonal range. Contrast is an expression of the rate of change of image density versus imaging energy. Depending on the end use of the image different parts of the image range have greater or lesser importance. For the material herein described the whole of the density range is important so the applicable measure of contrast is over the range of densities from the 'toe' (E1) or onset of image density, to the shoulder (E2) or onset of D max .
- the practical measure of E1 is the thermal energy which generates a density 0.1 greater than Dmin.
- the practical measure of E2 is the thermal energy that generates a density 90% of D max .
- the tonal range is the value of E2 - E1.
- the density of the image increases from a minimum (D min ) value to a maximum (D max ) value. It is desirable for the D min to be as low as possible and the D max to be high enough that pleasing image density is achieved. For a transmission image D min of less than 0.1 and D max of greater than 2.5 are considered acceptable.
- the dynamic range of the thermal imaging material is D max - D min .
- Tonal and dynamic ranges are given for the high activity reducing agents in Table 3.
- the amount of high activity reducing agent used in the thermal imaging material of this invention is preferably about 0.005 to about 0.2 millimoles/mole Ag, more preferably about 0.01 to about 0.1 and most preferable about 0.015 to about 0.05 mmoles/mole Ag.
- the amount of low activity reducing agent is preferably about 0.05 to about 2, more preferably about 0.1 to about 1 and most preferably .15 to about 0.5 mmoles/mole Ag.
- the ratio of the amount of high activity reducing agent to the amount of low activity reducing agent is about 1 to 3 to about 1 to 30, particularly preferred is a ratio of about 1 to about 10.
- the imaging composition and element of the invention can also contain a so-called activator-toning agent, also known as an accelerator-toning agent or toner.
- the activator-toning agent can be a cyclic imide and is typically useful in a range of concentration such as a concentration of about 0.10 mole to about 1.1 mole of activator -toning agent per mole of silver salt oxidizing agent in the thermographic material.
- Typical suitable activator-toning agents are described in Belgian Patent No. 766,590 issued June 15, 1971.
- Typical activator-toning agents include, for example, phthalimide, N-hydroxyphthalimide, N-hydroxy-1,8-naphthalimide, N-potassium phthalimide, N-mercury phthalimide, succinimide and/or N-hydroxysuccinimide. Combinations of activator-toning agents can be employed if desired. Other activator-toning agents which can be employed include phthalazinone, 2-acetyl-phthalazinone and the like.
- thermographic imaging composition of the invention can contain other addenda that aid in formation of a useful image.
- thermographic composition of the invention can contain various other compounds alone or in combination as vehicles, binding agents and the like, which can be in various layers of the thermographic element of the invention.
- Suitable materials can be hydrophobic or hydrophilic. They are transparent or translucent and include such synthetic polymeric substances as water soluble polyvinyl compounds like poly(vinyl pyrrolidone), acrylamide polymers and the like.
- Other synthetic polymeric compounds which can be employed include dispersed vinyl compounds such as in latex form and particularly those which increase dimensional stability of photographic materials.
- Effective polymers include water insoluble polymers of polyesters, polycarbonates, alkyl acrylates and methacrylates, acrylic acid, sulfoalkyl acrylates, methacrylates and those which have crosslinking sites which facilitate hardening or curing as well as those having recurring sulfobetaine units as described in Canadian Patent No. 774,054.
- Especially useful high molecular weight materials and resins include poly(vinyl acetals), such as, poly(vinyl acetal) and poly(vinyl butyral), cellulose acetate butyrate, polymethyl methacrylate, poly(vinyl pyrrolidone), ethylcellulose, polystyrene, polyvinyl chloride, chlorinated rubber, polyisobutylene, butadiene-styrene copolymers, vinyl chloride-vinyl acetate copolymers, copolymers, of vinyl acetate, vinyl chloride and maleic acid and polyvinyl alcohol.
- poly(vinyl acetals) such as, poly(vinyl acetal) and poly(vinyl butyral), cellulose acetate butyrate, polymethyl methacrylate, poly(vinyl pyrrolidone), ethylcellulose, polystyrene, polyvinyl chloride, chlorinated rubber, polyisobuty
- thermographic element according to the invention comprises a thermal imaging composition, as described above, on a support.
- supports can be used. Typical supports include cellulose nitrate film, cellulose ester film, poly(vinyl acetal) film, polystyrene film, poly(ethylene terephthalate) film, polycarbonate film and related films or resinous materials, as well as glass, paper, metal and the like supports which can withstand the processing temperatures employed according to the invention.
- a flexible support is employed.
- thermographic imaging elements of the invention can be prepared by coating the layers on a support by coating procedures known in the photographic art, including dip coating, air knife coating, curtain coating or extrusion coating using hoppers. If desired, two or more layers are coated simultaneously.
- Thermographic imaging elements are described in general in, for example, U.S. Patents 3,457,075; 4,459,350; 4,264,725 and 4,741,992 and Research Disclosure , June 1978, Item No. 17029.
- thermographic element can be in any location in the element that provides the desired image. If desired, one or more of the components can be in more than one layer of the element. For example, in some cases, it is desirable to include certain percentages of the reducing agent, toner, stabilizer and/or other addenda in an overcoat layer. This, in some cases, can reduce migration of certain addenda in the layers of the element.
- the thermographic imaging element of the invention can contain a transparent, image insensitive protective layer.
- the protective layer can be an overcoat layer, that is a layer that overlies the image sensitive layer(s), or a backing layer, that is a layer that is on the opposite side of the support from the image sensitive layer(s).
- the imaging element can contain both a protective overcoat layer and a protective backing layer, if desired.
- An adhesive interlayer can be imposed between the imaging layer and the protective layer and/or between the support and the backing layer.
- the protective layer is not necessarily the outermost layer of the imaging element.
- the protective overcoat layer preferably acts as a barrier layer that not only protects the imaging layer from physical damage, but also prevents loss of components from the imaging layer.
- the overcoat layer preferably comprises a film forming binder, preferable a hydrophilic film forming binder.
- binders include, for example, crosslinked polyvinyl alcohol, gelatin, poly(silicic acid), and the like. Particularly preferred are binders comprising poly(silicic acid) alone or in combination with a water-soluble hydroxyl-containing monomer or polymer as described in the above-mentioned US Patent No. 4,828,971.
- thermographic imaging element of this invention can include a backing layer.
- the backing layer is an outermost layer located on the side of the support opposite to the imaging layer. It is typically comprised of a binder and a matting agent which is dispersed in the binder in an amount sufficient to provide the desired surface roughness and the desired antistatic properties.
- the backing layer should not adversely affect sensitometric characteristics of the thermographic element such as minimum density, maximum density and photographic speed.
- thermographic element of this invention preferably contains a slipping layer to prevent the imaging element from sticking as it passes under the thermal print head.
- the slipping layer comprises a lubricant dispersed or dissolved in a polymeric binder.
- Lubricants the can be used include, for example:
- thermographic imaging elements of this invention can contain either organic or inorganic matting agents.
- organic matting agents are particles, often in the form of beads, of polymers such as polymeric esters of acrylic and methacrylic acid, e.g., poly(methylmethacrylate), styrene polymers and copolymers, and the like.
- inorganic matting agents are particles of glass, silicon dioxide, titanium dioxide, magnesium oxide, aluminum oxide, barium sulfate, calcium carbonate, and the like. Matting agents and the way they are used are further described in U.S. Patent Nos. 3,411,907 and 3,754,924.
- the concentration of matting agent required to give the desired roughness depends on the mean diameter of the particles and the amount of binder. Preferred particles are those with a mean diameter of from about 1 to about 15 micrometers, preferably from 2 to 8 micrometers.
- the matte particles can be usefully employed at a concentration of about 1 to about 100 milligrams per square meter.
- the imaging element can also contain an electroconductive layer which, in accordance with US 5,310,640, is an inner layer that can be located on either side of said support.
- the electroconductive layer preferably has an internal resistivity of less than 5 x 10 11 ohms/square.
- the protective overcoat layer and the slipping layer may either or both be electrically conductive having a surface resistivity of less than 5 x 10 11 ohms/square.
- electrically conductive overcoat layers are described in US Patent No. 5,547,821.
- electrically conductive overcoat layers comprise metal-containing particles dispersed in a polymeric binder in an amount sufficient to provide the desired surface resistivity. Examples of suitable electrically-conductive metal-containing particles for the purposes of this invention include:
- thermographic elements and compositions of this invention.
- a support of polyethylene terephthalate having a thickness of 178 micron was doctor blade coated from a coating composition containing methyl ethyl ketone as solvent and the listed components so as to give the final dry weights as shown.
- SILVER BEHENATE 400 mg/sq.ft (4.4 g/m 2 ) POLYVINYL ACETAL 400 mg/sq.ft (4.4 g/m 2 ) PHTHALAZINONE 40 mg/sq.ft (.44 g/m 2 ) REDUCING AGENT 1 AS LISTED mg/sq.ft (g/m 2 ) REDUCING AGENT 2 AS LISTED mg/sq.ft (g/m 2 )
- Dynamic range is simply D max - D min .
- Tonal Range is E2 - E1 expressed in units of pulse count.
- Table 4 sets forth the reducing agents used, the amounts of reducing agents and the dynamic and tonal ranges obtained.
- each of the strong reducing agents is combined with each of the weak reducing agents as defined in Table 4.
- the dynamic and tonal range of the mixture is greater than the sum of the strong reducing agent by itself and the weak reducing agent by itself.
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- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Non-Silver Salt Photosensitive Materials And Non-Silver Salt Photography (AREA)
- Thermal Transfer Or Thermal Recording In General (AREA)
- Heat Sensitive Colour Forming Recording (AREA)
Abstract
A thermographic imaging element comprises:
Description
The present invention relates to
thermographic compositions and elements for use in
direct thermal imaging.
Thermal imaging is a process in which images
are recorded by the use of imagewise modulated thermal
energy. In general there are two types of thermal
recording processes, one in which the image is
generated by thermally activated transfer of a light
absorbing material, the other generates the light
absorbing species by thermally activated chemical or
physical modification of components of the imaging
medium. A review of thermal imaging methods is found in
"Imaging Systems" by K.I. Jacobson R.E.Jacobson -
Focal Press 1976.
Thermal energy can be delivered in a number
of ways, for example by direct thermal contact or by
absorption of electromagnetic radiation. Examples of
radiant energy include infrared lasers. Modulation of
thermal energy can be by intensity or duration or both.
For example a thermal print head comprising microscopic
resistor elements is fed pulses of electrical energy
which are converted into heat by the Joule effect. In a
particularly useful embodiment the pulses are of fixed
voltage and duration and the thermal energy delivered
is then controlled by the number of such pulses sent.
Radiant energy can be modulated directly by means of
the energy source e.g. the voltage applied to a solid
state laser.
Direct imaging by chemical change in the
imaging medium usually involves an irreversible
chemical reaction which takes place very rapidly at
elevated temperatures - say above 100°C - but at room
temperature the rate is orders of magnitude slower such
that effectively the material is stable.
A particularly useful direct thermal imaging
element uses an organic silver salt in combination with
a reducing agent. Such systems are often referred to as
'dry silver'. In this system the chemical change
induced by the application of thermal energy is the
reduction of the transparent silver salt to a metallic
silver image.
Prior art thermal imaging elements tend to
have a relatively low dynamic range or relatively a
narrow latitude which limits the number of tones or
levels of gray that can be recorded.
One aspect of this invention comprises a
thermographic imaging element comprising:
This invention provides a heat-sensitive
recording material suitable for direct thermal imaging
having a high dynamic range (Dmax ≥ 2.5, Dmin ≤ 0.1, as
described hereinafter) and a wide latitude (E1 - E2, as
described hereinafter) such that a large number of
tones or levels of gray can be recorded.
Figure 1 shows the characteristic
sensitometric curves obtained by plotting image density
(D) versus the imaging thermal energy expressed as the
number of thermal pulses applied. Labels identify the
examples as high activity (H1 through H5) and low
activity (L1 through L3) as shown in Tables 1 & 2.
Figure 2 shows a sensitometric curve showing
E1, E2, Dmin and Dmax.
Figures 3 - 7 show sensitometric curves
obtained, as set forth in more detail below, from
thermographic imaging materials in accordance with this
invention (D1 through D15) and comparison materials (C1
through C5).
The thermographic element and composition
according to the invention comprise an oxidation-reduction
image-forming composition which contains a
silver salt, a high activity reducing agent, as defined
herein) and a low activity reducing agent ( as defined
herein).
The oxidizing agent is preferably a silver salt.
of an organic acid. Suitable silver salts include, for
example, silver behenate, silver stearate, silver
oleate, silver laureate, silver hydroxy stearate,
silver caprate, silver myristate, silver palmitate
silver benzoate, silver benzotriazole, silver
terephthalate, silver phthalate saccharin silver,
phthalazionone silver, benzotriazole silver, silver
salt of 3-(2-carboxyethyl-4-4-hydroxymethyl-4-thiazoline-2-thione,
silver salt of 3- mercapto-4-phenyl-1,2,4-triazole
and the like. In most instances
silver behenate is most useful.
A variety of reducing agents can be employed
in the imaging composition of the invention. Typical
reducing agents which can be used include, for example:
To determine the activity of a reducing agent
the following procedure is conducted. A test
formulation containing the following activity
formulation # 1 is prepared.
| |
SILVER BEHENATE | 0.88 millimole/sq.ft. (9.7 millimole/sq.m.) |
POLY(VINYL BUTYRAL) | 400 mg/sq.ft. (4400mg/ sq.m.) |
SUCCINIMIDE | 0.25 millimole/sq.ft. (2.75 millimole/ sq.m.) |
TEST REDUCING AGENT | 0.75 millimole / sq. ft. (8.25 millimole/ sq.m.) |
The formulation is coated on a support and is
thermally imaged using a thin film thermal head in
contact with a combination of the imaging medium and a
protective film of 6 micron thickness polyester sheet.
Contact of the head to the element is maintained by an
applied pressure of 313 g/cm heater line. The line
write time is 15 millisec. broken up into 255
increments corresponding to the pulse width referred to
above. Energy per pulse is 0.041 Joule/sq.cm.
Individual picture elements are of a size corresponding
to 300 dots per inch.
The thermal sensitive coatings are treated
with a linearly increasing pattern of pulses from 5 to
255 in 10 pulse increments. Densities of the resulting
image steps are measured with an X-Rite 361
densitometer in the 'ortho' mode. In the activity
determination for low activity reducing agents, an
additional test in which the average printing energy
per pulse is increased to 0.085 Joules per sq. cm is
required to generate sufficient density in the case of
the low activity reducing agents. Measured activity
values for high activity reducing agents, are the same
in both tests. Plots of density versus pulse count can
then be generated and the activity, E1, the 'toe' of
the curve, i.e., the onset of image density, can be
read from the plot. The practical measure of E1 is the
thermal energy which generates a density 0.1 greater
than Dmin. Energies can be converted from pulse count
to Joules/sq.cm. using the factors given above.
Preferred high activity reducing agents have
an activation energy of less than about 6 Joules/sq.
cm. In preferred embodiments of the invention, the
high activity reducing agent has an activation energy
between about 1 and 10 Joules/sq. cm. and preferably
between about 3 and about 6 Joules/sq. cm.
Low activity reducing agents have an
activity, as defined herein, of equal to or greater
than 10 Joules/sq. cm. The low activity reducing
agents preferably have an activity between about 10 and
about 20 Joules/sq. cm., more preferably between about
10 and about 15 Joules/sq.cm.
Plots of the density versus pulse count for
all the reducing agents of Tables 1 & 2 are given in
Figure 1. Figure 1 shows the characteristic
sensitometric curves obtained by plotting image density
(D) versus the imaging thermal energy expressed as the
number of thermal pulses applied. Labels identify the
examples as high activity (H1 through H5) and low
activity (L1 through L3) as shown in Tables 1 & 2.
From the same plots of density versus pulse
count, the Dmax, Dmin, E1, and E2 values, as described
below and in Figure 2, can also be obtained. The plots
of density versus pulse count also provides contrast
and tonal range. Contrast is an expression of the rate
of change of image density versus imaging energy.
Depending on the end use of the image different parts
of the image range have greater or lesser importance.
For the material herein described the whole of the
density range is important so the applicable measure of
contrast is over the range of densities from the 'toe'
(E1) or onset of image density, to the shoulder (E2) or
onset of Dmax. The practical measure of E1 is the
thermal energy which generates a density 0.1 greater
than Dmin. Similarly the practical measure of E2 is
the thermal energy that generates a density 90% of Dmax.
The tonal range is the value of E2 - E1.
Under the action of the applied thermal
energy the density of the image increases from a
minimum (Dmin) value to a maximum (Dmax) value. It is
desirable for the Dmin to be as low as possible and the
Dmax to be high enough that pleasing image density is
achieved. For a transmission image Dmin of less than
0.1 and Dmax of greater than 2.5 are considered
acceptable. The dynamic range of the thermal imaging
material is Dmax - Dmin.
Tonal and dynamic ranges are given for the
high activity reducing agents in Table 3.
Single Reducing Agent Dynamic & Tonal Range | ||
Reducing Agent | Dynamic Range (Δ density) | Tonal Range (pulse count) |
H1 | 2.46 | 68 |
H2 | 1.71 | 84 |
H3 | 2.21 | 82 |
H4 | 2.97 | 63 |
H5 | 2.6 | 51 |
The amount of high activity reducing agent
used in the thermal imaging material of this invention
is preferably about 0.005 to about 0.2 millimoles/mole
Ag, more preferably about 0.01 to about 0.1 and most
preferable about 0.015 to about 0.05 mmoles/mole Ag.
The amount of low activity reducing agent is preferably
about 0.05 to about 2, more preferably about 0.1 to
about 1 and most preferably .15 to about 0.5
mmoles/mole Ag. Typically the ratio of the amount of
high activity reducing agent to the amount of low
activity reducing agent is about 1 to 3 to about 1 to
30, particularly preferred is a ratio of about 1 to
about 10.
The imaging composition and element of the
invention can also contain a so-called activator-toning
agent, also known as an accelerator-toning agent or
toner. The activator-toning agent can be a cyclic
imide and is typically useful in a range of
concentration such as a concentration of about 0.10
mole to about 1.1 mole of activator -toning agent per
mole of silver salt oxidizing agent in the
thermographic material. Typical suitable activator-toning
agents are described in Belgian Patent No.
766,590 issued June 15, 1971. Typical activator-toning
agents include, for example, phthalimide, N-hydroxyphthalimide,
N-hydroxy-1,8-naphthalimide, N-potassium
phthalimide, N-mercury phthalimide,
succinimide and/or N-hydroxysuccinimide. Combinations
of activator-toning agents can be employed if desired.
Other activator-toning agents which can be employed
include phthalazinone, 2-acetyl-phthalazinone and the
like.
The thermographic imaging composition of the
invention can contain other addenda that aid in
formation of a useful image.
A thermographic composition of the invention
can contain various other compounds alone or in
combination as vehicles, binding agents and the like,
which can be in various layers of the thermographic
element of the invention. Suitable materials can be
hydrophobic or hydrophilic. They are transparent or
translucent and include such synthetic polymeric
substances as water soluble polyvinyl compounds like
poly(vinyl pyrrolidone), acrylamide polymers and the
like. Other synthetic polymeric compounds which can be
employed include dispersed vinyl compounds such as in
latex form and particularly those which increase
dimensional stability of photographic materials.
Effective polymers include water insoluble polymers of
polyesters, polycarbonates, alkyl acrylates and
methacrylates, acrylic acid, sulfoalkyl acrylates,
methacrylates and those which have crosslinking sites
which facilitate hardening or curing as well as those
having recurring sulfobetaine units as described in
Canadian Patent No. 774,054. Especially useful high
molecular weight materials and resins include
poly(vinyl acetals), such as, poly(vinyl acetal) and
poly(vinyl butyral), cellulose acetate butyrate,
polymethyl methacrylate, poly(vinyl pyrrolidone),
ethylcellulose, polystyrene, polyvinyl chloride,
chlorinated rubber, polyisobutylene, butadiene-styrene
copolymers, vinyl chloride-vinyl acetate copolymers,
copolymers, of vinyl acetate, vinyl chloride and maleic
acid and polyvinyl alcohol.
A thermographic element according to the
invention comprises a thermal imaging composition, as
described above, on a support. A wide variety of
supports can be used. Typical supports include
cellulose nitrate film, cellulose ester film,
poly(vinyl acetal) film, polystyrene film,
poly(ethylene terephthalate) film, polycarbonate film
and related films or resinous materials, as well as
glass, paper, metal and the like supports which can
withstand the processing temperatures employed
according to the invention. Typically, a flexible
support is employed.
The thermographic imaging elements of the
invention can be prepared by coating the layers on a
support by coating procedures known in the photographic
art, including dip coating, air knife coating, curtain
coating or extrusion coating using hoppers. If
desired, two or more layers are coated simultaneously.
Thermographic imaging elements are described
in general in, for example, U.S. Patents 3,457,075;
4,459,350; 4,264,725 and 4,741,992 and Research
Disclosure, June 1978, Item No. 17029.
The components of the thermographic element
can be in any location in the element that provides the
desired image. If desired, one or more of the
components can be in more than one layer of the
element. For example, in some cases, it is desirable
to include certain percentages of the reducing agent,
toner, stabilizer and/or other addenda in an overcoat
layer. This, in some cases, can reduce migration of
certain addenda in the layers of the element.
The thermographic imaging element of the
invention can contain a transparent, image insensitive
protective layer. The protective layer can be an
overcoat layer, that is a layer that overlies the image
sensitive layer(s), or a backing layer, that is a layer
that is on the opposite side of the support from the
image sensitive layer(s). The imaging element can
contain both a protective overcoat layer and a
protective backing layer, if desired. An adhesive
interlayer can be imposed between the imaging layer and
the protective layer and/or between the support and the
backing layer. The protective layer is not necessarily
the outermost layer of the imaging element.
The protective overcoat layer preferably acts
as a barrier layer that not only protects the imaging
layer from physical damage, but also prevents loss of
components from the imaging layer. The overcoat layer
preferably comprises a film forming binder, preferable
a hydrophilic film forming binder. Such binders
include, for example, crosslinked polyvinyl alcohol,
gelatin, poly(silicic acid), and the like.
Particularly preferred are binders comprising
poly(silicic acid) alone or in combination with a
water-soluble hydroxyl-containing monomer or polymer as
described in the above-mentioned US Patent
No. 4,828,971.
The thermographic imaging element of this
invention can include a backing layer. The backing
layer is an outermost layer located on the side of the
support opposite to the imaging layer. It is typically
comprised of a binder and a matting agent which is
dispersed in the binder in an amount sufficient to
provide the desired surface roughness and the desired
antistatic properties.
The backing layer should not adversely affect
sensitometric characteristics of the thermographic
element such as minimum density, maximum density and
photographic speed.
The thermographic element of this invention
preferably contains a slipping layer to prevent the
imaging element from sticking as it passes under the
thermal print head. The slipping layer comprises a
lubricant dispersed or dissolved in a polymeric binder.
Lubricants the can be used include, for example:
In the thermographic imaging elements of this
invention can contain either organic or inorganic
matting agents. Examples of organic matting agents are
particles, often in the form of beads, of polymers such
as polymeric esters of acrylic and methacrylic acid,
e.g., poly(methylmethacrylate), styrene polymers and
copolymers, and the like. Examples of inorganic
matting agents are particles of glass, silicon dioxide,
titanium dioxide, magnesium oxide, aluminum oxide,
barium sulfate, calcium carbonate, and the like.
Matting agents and the way they are used are further
described in U.S. Patent Nos. 3,411,907 and 3,754,924.
The concentration of matting agent required
to give the desired roughness depends on the mean
diameter of the particles and the amount of binder.
Preferred particles are those with a mean diameter of
from about 1 to about 15 micrometers, preferably from 2
to 8 micrometers. The matte particles can be usefully
employed at a concentration of about 1 to about 100
milligrams per square meter.
The imaging element can also contain an
electroconductive layer which, in accordance with US
5,310,640, is an inner layer that can be located on
either side of said support. The electroconductive
layer preferably has an internal resistivity of less
than 5 x 1011 ohms/square.
The protective overcoat layer and the
slipping layer may either or both be electrically
conductive having a surface resistivity of less than
5 x 1011 ohms/square. Such electrically conductive
overcoat layers are described in US Patent No.
5,547,821. As taught in the 821 patent, electrically
conductive overcoat layers comprise metal-containing
particles dispersed in a polymeric binder in an amount
sufficient to provide the desired surface resistivity.
Examples of suitable electrically-conductive metal-containing
particles for the purposes of this invention
include:
The following examples illustrate the
thermographic elements and compositions of this
invention.
A support of polyethylene terephthalate
having a thickness of 178 micron was doctor blade
coated from a coating composition containing methyl
ethyl ketone as solvent and the listed components so as
to give the final dry weights as shown.
SILVER BEHENATE | 400 mg/sq.ft (4.4 g/m2) |
POLYVINYL ACETAL | 400 mg/sq.ft (4.4 g/m2) |
PHTHALAZINONE | 40 mg/sq.ft (.44 g/m2) |
REDUCING | AS LISTED mg/sq.ft (g/m2) |
REDUCING AGENT 2 | AS LISTED mg/sq.ft (g/m2) |
Coatings were imaged using the procedure
defined above. Dynamic range is simply Dmax - Dmin. Tonal
Range is E2 - E1 expressed in units of pulse count.
Table 4 sets forth the reducing agents used, the
amounts of reducing agents and the dynamic and tonal
ranges obtained.
Reducing agent Mixtures - Dynamic & Tonal Range | ||||||
EXAMPLE ID | REDUCING AGENT 1 | REDUCING AGENT 2 | DYNAMIC RANGE | TONAL RANGE | ||
ID | AMT | ID | AMT | |||
C1 | H1 | 10 (0.11) | - | - | 0.93 | 41 |
D1 | H1 | 10 (0.11) | L1 | 100 (1.1) | 2.95 | 92 |
D2 | H1 | 10 (0.11) | L2 | 320 (3.5) | 2.63 | 73 |
D3 | H1 | 10 (0.11) | L3 | 180 (2.0) | 1.99 | 82 |
C2 | H2 | 8 (0.08) | - | - | 0.76 | 87 |
D4 | H2 | 8 (0.08) | L1 | 100 (1.1) | 2.47 | 113 |
D5 | H2 | 8 (0.08) | L2 | 280 (3.1) | 2.66 | 107 |
D6 | H2 | 8 (0.08) | L3 | 140 (1.5) | 2.51 | 124 |
C3 | H3 | 20 (0.22) | - | - | 0.96 | 56 |
D7 | H3 | 20 (0.22) | L1 | 100 (1.1) | 2.74 | 121 |
D8 | H3 | 20 (0.22) | L2 | 320 (3.5) | 2.68 | 106 |
D9 | H3 | 20 (0.22) | L3 | 180 (2.0) | 2.09 | 126 |
C4 | H4 | 10 (0.11) | - | - | 0.85 | 39 |
D10 | H4 | 10 (0.11) | L1 | 100 (1.1) | 2.6 | 78 |
D11 | H4 | 10 (0.11) | L2 | 320 (3.5) | 2.01 | 91 |
D12 | H4 | 10 (0.11) | L3 | 180 (2.0) | 1.77 | 80 |
C5 | H5 | 10 (0.11) | - | - | .82 | 35 |
D13 | H5 | 10 (0.11) | L1 | 100 (1.1) | 2.12 | 106 |
D14 | H5 | 10 (0.11) | L2 | 320 (3.5) | 2.64 | 82 |
D15 | H5 | 10 (0.11) | L3 | 180 (2.0) | 1.93 | 104 |
In Figures 3-7 each of the strong reducing
agents is combined with each of the weak reducing
agents as defined in Table 4. In every case the dynamic
and tonal range of the mixture is greater than the sum
of the strong reducing agent by itself and the weak
reducing agent by itself.
The invention has been described in detail
with particular reference to preferred embodiments, but
it will be understood that variations and modifications
can be effected within the spirit and scope of the
invention.
Claims (10)
- A thermographic imaging element comprising:(a) a support;(b) an imaging layer comprising:(i) a silver salt;(ii) a first reducing agent which has high activity with an activation energy of less than 10 Joules/sq.cm.; and(iii) a second reducing agent which has low activity with an activation energy of greater than or equal to 10 Joules/sq. cm.
- An imaging element according to claim any preceding claim, wherein the high activity reducing agent is present in an amount of about 0.005 to about 0.2 mmoles/mole Ag.
- An imaging element according to claim any preceding claim, wherein the low activity reducing agent is present in an amount of about 0.05 to about 2 mmoles/mole Ag.
- An imaging element according to any preceding claim, wherein the ratio of the amount of high activity reducing agent to the amount of low activity reducing agent is about 1 to 3 to about 1 to 30.
- A composition comprising:(i) a silver salt;(ii) a first reducing agent which has high activity with an activation energy of less than 10 Joules/sq. cm.; and(iii) a second reducing agent which has low activity with an activation energy of greater than or equal to 10 Joules/sq. cm.
- A composition according to claim 9, wherein the ratio of the amount of high activity reducing agent to the amount of low activity reducing agent is about 1 to 3 to about 1 to 30.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US08/770,750 US6066445A (en) | 1996-12-19 | 1996-12-19 | Thermographic imaging composition and element comprising said composition |
US770750 | 1996-12-19 |
Publications (1)
Publication Number | Publication Date |
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EP0849625A1 true EP0849625A1 (en) | 1998-06-24 |
Family
ID=25089570
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP97203852A Withdrawn EP0849625A1 (en) | 1996-12-19 | 1997-12-08 | Thermographic imaging composition and element comprising said composition |
Country Status (3)
Country | Link |
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US (1) | US6066445A (en) |
EP (1) | EP0849625A1 (en) |
JP (1) | JPH10203011A (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0943960A1 (en) * | 1998-03-20 | 1999-09-22 | Eastman Kodak Company | Thermographic imaging element |
EP0943959A1 (en) * | 1998-03-20 | 1999-09-22 | Eastman Kodak Company | Thermographic imaging element |
EP0943958A1 (en) * | 1998-03-20 | 1999-09-22 | Eastman Kodak Company | Thermographic imaging element |
EP0943957A1 (en) * | 1998-03-20 | 1999-09-22 | Eastman Kodak Company | Thermographic imaging element |
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EP0582144A1 (en) * | 1992-08-03 | 1994-02-09 | Minnesota Mining And Manufacturing Company | Laser addressable thermal recording material |
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FR2089285A5 (en) * | 1970-04-09 | 1972-01-07 | Agfa Gevaert Nv | |
US4082901A (en) * | 1973-04-04 | 1978-04-04 | Agfa-Gevaert N.V. | Thermographic material |
CA1020347A (en) * | 1973-04-04 | 1977-11-08 | Urbain L. Laridon | Thermographic process and material |
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EP0943959A1 (en) * | 1998-03-20 | 1999-09-22 | Eastman Kodak Company | Thermographic imaging element |
EP0943958A1 (en) * | 1998-03-20 | 1999-09-22 | Eastman Kodak Company | Thermographic imaging element |
EP0943957A1 (en) * | 1998-03-20 | 1999-09-22 | Eastman Kodak Company | Thermographic imaging element |
Also Published As
Publication number | Publication date |
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JPH10203011A (en) | 1998-08-04 |
US6066445A (en) | 2000-05-23 |
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